HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → HCID 814117, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-Nitrobenzenesulfonyl chloride | HCID 15540 | — |
| Reactant | 3,4-Dimethoxyaniline | HCID 22770 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 814117 | HCID 814117 | 54.7% |
Reaction Steps
A mixture of 2-nitrobenzenesulfonyl chloride (3.0 g, 13.5 mmol) and 3,4-dimethoxyaniline (2.1 g, 14.9 mmol) in 1,4-dioxane (30 mL) in a sealed reaction tube was heated at 80° C. for 24 h with TLC monitoring (hexane: EtOAc, 1:1). The reaction mixture was diluted with H2O (30 mL), extracted with EtOAc (3×100 mL) and the combined organic phases dried over Na2SO4, filtered and concentrated in vacuo. Purification by gradient flash chromatography, eluting with 20-25% EtOAc in hexane yielded the title compound (2.5 g, 7.39 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249160B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-8d9e535e024b46e69dc42f6a493a1e6e |
| Source note | uspto-grants-2016_02 |